The reaction of molten phenylphosphonic acid with a layered double hydroxide and its calcined oxide

The reaction of molten phenylphosphonic acid with a layered double hydroxide and its calcined oxide

Phenylphosphonic acid was thermally intercalated into both the host Mg-Al-CO 3 layered double hydroxide (LDH) and its corresponding oxide material (LDO) formed by the thermal decomposition of the host LDH via a novel slow heating method. In the thermal intercalation process, the host and guest react...

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Bibliographic Details
Published in:Solid state ionics Vol. 84; no. 1; pp. 117 - 129
Main Authors: Carlino, Simon, Hudson, Michael J., Husain, S.Waqif, Knowles, James A.
Format: Journal Article
Language:English
Published: Amsterdam Elsevier B.V 01-03-1996
Elsevier Science
Subjects:
Chemistry
Exact sciences and technology
Inorganic chemistry and origins of life
Layered double hydroxide (LDH)
Layered double oxide (LDO)
Miscellaneous
Phenylphosphonic acid
Preparations and properties
Phenylphosphonic acid
Layered double hydroxide (LDH)
Layered double oxide (LDO)
Pyrolysis
Aluminium Hydroxides
Thermogravimetry
Differential thermal analysis
X ray diffraction
Phosphorus Organic compounds
Molten salt
Intercalation compound
Lamellar structure
Quaternary compound
Magnesium Hydroxides
Infrared spectrum
Melting point
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Summary:Phenylphosphonic acid was thermally intercalated into both the host Mg-Al-CO 3 layered double hydroxide (LDH) and its corresponding oxide material (LDO) formed by the thermal decomposition of the host LDH via a novel slow heating method. In the thermal intercalation process, the host and guest reactants are carefully heated together to a temperature just above the melting point of the guest. The resulting intercalation compounds were studied by a variety of analytical techniques. Powder X-ray diffraction (PXRD) indicated that the reaction products were all polyphasic microcrystalline materials and suggested that arrangement of the phenylphosphonate anions between the LDH and LDO layers was similar to that exhibited by zirconium (IV) bis(benzenephosphonate), α-Zr(C 6H 5PO 3) 2 formed via a topotactic reaction. Fourier-transformed infrared (FTIR) was inconclusive, while thermal analysis of the reaction mixture clearly showed the reaction taking place. 27Al, 13C and 31P solid-state magic-angle spinning nuclear magnetic resonance (MAS NMR) indicated the presence of the anion of phenylphosphonic acid together with some free/unintercalated acid. Collectively, these techniques suggested that the phosphonic acid was intercalated between the layers of both LDH and LDO hosts by way of an acid-base condensation reaction.
ISSN:0167-2738
1872-7689
DOI:10.1016/S0167-2738(96)83014-1